INSTRUCTION MANUAL.

CSTR
SET UP
DESCRIPTION
SPECIFICATIONS
INSTALLATION REQUIRMENTS
INSTALLATION AND CONNECTIONS
PRECAUTIONS
TROUBLE SHOOTING

EXPREMENTATION
THEORY
OPERATING PROCEDURE
SYSTEM CONSTANTS
OBSERVATION TABLE
CALCULATIONS

CSTR
AIM:
To study the saponification of ethyl acetate in a constant flow stirrer tank
reactor and to determine percentage conversion and theoretical conversion.
APPARATUS:
A CSTR setup, burette, pipette, conical flasks. Measuring cylinders etc.
CHEMICALS :
Ethyl acetate, NaOH, oxalic acid, HCl, phenolphthalein indicator
THEORY:
Saponification of ethyl acetate undergoes as follows:
CH3COOC2H5 + NaOH CH3COONa + C2H5OH
B

Reaction is made homogeneous and is first order with respect to ester and
alkali. The rate of reaction can therefore be written as,
-rA = KCACB

K = 10 lit/gm mole.min at 25 deg. C

Performance equation of the constant flow stirred tank reactor is

(VCAO /FAO) =

= (CAO XA) / [ K CAO (1 XA) (M-XA)]

K CAO = XA/ (1 - XA) (M - XA) ------- (1) M= CBO / CAO

when M 1

PROCEDURE:
Prepare the following solutions:
Ethyl acetate 0.1 N, NaOH 0.05N, HCl/Acetic acid -0.05 N
All solutions are prepared freshly and standerdise NaOH with oxalic acid. The
experiment is to be carried out at room temperature. Fill up the feed tanks
with 5 liters of NaOH and ethyl acetate. Find out the volume of the reactor.
Adjust total flow rate into the reactor in such a way to have residence time of
4-5 min.

Collect the samples after 2

time. At interval of 5 min collect 4-5

samples. Titrate the sample against HCl immediately (as the reaction is very
fast experiment is carried out without arrestation.)
For steady state to be approached a low 2

to 3

time to be elapsed

before taking samples for titration.

Volume of reactor is 1 liter.
Operating procedure

1. Feed tanks open small air vent valve and insure that bottom valves
are closed. Fill up feed tanks slowly. Close all valves of feed tank.

2. Start air supply to both the tanks through air regulator, assuring that
the air pressure from regulator to feed tanks will not exceed 1 to 1.5
kg/cm.

3. Slowly open feed valve say 25% open.

4. Adjust Rota meter valves to desired flows and ensure steady-state flow
rate.

5. Initially keep minimum flow rates possible.

6. After reaching to steady-state of process conditions start to withdraw
samples.

7. After experimentation first close air supply valve to tanks.

8. Drain all tanks slowly.
9. Flush all system tanks and vessels by circulating water through it.

10. Important note: during pneumatic conveying, dont allow air to pass
through Rota meters from feed tank. It may damage Rota meter tube.
So ensure sufficient quantity of feed material in feed tanks.

OBSERVATION:
Volume of reactor = V
Vol. Flow rate of ester = VB
Vol. flow rate of NaOH = VA
Normality of ester = CBO
Normality of NaOH = CAO
Normality of oxalic acid = NOX
Normality of HCl = NHCl
Sr. No.

Time ( min)

Burette reading ( VHCl)

CALCULATIONS:
= V / (VA + VB)
CA = NHCl VHCl / V sample
CAO = CAO CA) / CAO
X CAO

= (CAO CA) / CAO.

Theoretical conversion can be calculated by

K CAO

= XA / (1 XA) (M-XA) ------ (1)

M = CBO / CAO when M 1

RESULT:
The saponification of ethyl acetate in CSTR is studied and
1. Experimental conversion =
2. Theoretical conversion =